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Topic: Short Question Thread 2.0 (Read 5704 times)

Electro´S

Pupae

Posts: 95

Re: Short Question Thread 2.0

« Reply #340 on: March 30, 2013, 02:14:50 AM »

Finally i think. He wants say a balanced addition funnel instead of soxhlet capsule.It would be a RBF with the ethanol nitrostyrene mix at reflux with the NaBH4 in the funnel and the condenser at the top of the funnel.Then the NaBH4 is added to the reaction dissolved in the condensed ethanol drops.

Electro´S

Pupae

Posts: 95

Re: Short Question Thread 2.0

« Reply #341 on: March 30, 2013, 02:23:57 AM »

Ok, ok. This guy is talking about break the syphon part from a Soxhlet capsule. He he, i had need a little of time .

Tsathoggua

Autistic sociopath

Foundress Queen

Posts: 662

Re: Short Question Thread 2.0

« Reply #342 on: March 30, 2013, 02:59:10 AM »

Can HBr (room temp, 15% in GAA) be used successfully for ether cleavage of oxycodone to oxymorphone? if so, what are the yields like?

And my other quick question is this-Toady has been told on here that oxycodone esters are not worth bothering with. Does the same hold true for 6-position esters, or 3,6-diesters of oxymorphone? (talking about the enol ester here at the 3-position carbonyl)

« Last Edit: March 30, 2013, 04:06:36 AM by Tsathoggua »

Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

b6baddawg

Larvae

Posts: 35

Re: Short Question Thread 2.0

« Reply #343 on: April 02, 2013, 01:09:10 AM »

Am i missing something or can tma-2 be gotton too following this,veratraldehyde (3,4-dimethoxybenzaldehyde) > to (2-Bromo-4,5-dimethoxybenzaldehyde) > to 2,4,5-Trimethoxyphenyl-2-nitropropene > tma-2?

bjuice

Pupae

Posts: 59

Re: Short Question Thread 2.0

« Reply #344 on: April 09, 2013, 08:16:14 PM »

Hello Vespiary!

Just finished my first al/hg nitro reduction and am a little concerned because my toluene extraction came out with a deep yellow colour, whereas the pictorials I've seen both have their extractions come out colorless. So I'm assuming unreacted mdp2p, or maybe some other reaction byproducts. The reaction itself, as far as I can tell, went exactly as it should.

Either way, I'm conflicted on how to best work this up. I've already done my washes and have the organic layer drying over cacl2 at the moment. Now I'm trying to decide between

bjuice

Re: Short Question Thread 2.0

Just finished my first al/hg nitro reduction and am a little concerned because my toluene extraction came out with a deep yellow colour, whereas the pictorials I've seen both have their extractions come out colorless. So I'm assuming unreacted mdp2p, or maybe some other reaction byproducts. The reaction itself, as far as I can tell, went exactly as it should.

Either way, I'm conflicted on how to best work this up. I've already done my washes and have the organic layer drying over cacl2 at the moment. Now I'm trying to decide between

Gassed the toluene and....crystals! A whopping 3 grams from 45 grams mdp2p. I'm stoked that I've produced my first ever MDMA, but sad at the low yields. Luckily I'm working through another batch as we speak.

I'm going to wash the toluene with water in hopes that it's not completely dry, and has MDMA locked up in it.

zgoat65

Subordinate Wasp

Posts: 103

Re: Short Question Thread 2.0

« Reply #347 on: April 10, 2013, 12:48:55 AM »

Maybe add some bisulfite or metabisulfite to see if you have any ketone present. Also a good way to seperate.

If you build a man a fire, he'll be warm for a day.If you set a man on fire, he'll be warm for the rest of his life

bjuice

Pupae

Posts: 59

Re: Short Question Thread 2.0

« Reply #348 on: April 10, 2013, 12:59:28 AM »

Don't have any bisulfite on hand, but..

The water wash is looking GOOD. The aqueous layer instantly became cloudy as I watched crystal cascade from the organic layer to the aqueous. Scratch what I said about evaporating. Going to wash aqueous with clean toluene, separate, then basify the water to see if any oil drops out.

« Last Edit: April 10, 2013, 01:09:31 AM by bjuice »

bjuice

Pupae

Posts: 59

Re: Short Question Thread 2.0

« Reply #349 on: April 10, 2013, 01:30:48 AM »

Added NaOH to the water and it turned to what appears to be milk. Going to let it sit.

Aaand I'm accidentally rolling. Remind me to wear gloves next time I scrape the filter paper

Guess I'll be reporting back later with results. Any input on the workup situation would be greatly appreciated!

bjuice

Pupae

Posts: 59

Re: Short Question Thread 2.0

« Reply #350 on: April 10, 2013, 02:24:35 AM »

Washed the milky aqueous layer with clean toluene and a horrible looking emulsion formed, complete with what appears to be small plasticky flakes that won't dissolve in either layer. I think I may be beating a dead horse here

Edit: Separated layers and discarded aqueous. Filtered toluene through a buchner to remove the polymerized crap. Washed with 10% HCl/H2O, which is now evaporating. Don't wanna take my chances with gassing again.

« Last Edit: April 10, 2013, 03:44:34 AM by bjuice »

fractal

Subordinate Wasp

Posts: 110

Re: Short Question Thread 2.0

« Reply #351 on: April 10, 2013, 03:40:57 PM »

Sounds like you had some amine in your HCl/Water layer. Should have just evaporated of the water and recrystallized.

Flight

Larvae

Posts: 23

Re: Short Question Thread 2.0

« Reply #352 on: April 10, 2013, 07:56:30 PM »

I need some help understanding this, "Place the safrole (purified by simple distillation under vacuum) along with 2-5% KOH under good stirring. I use about 2.5% and it works like a charm."

bjuice

Re: Short Question Thread 2.0

Agreed. The aqueous layer finished evaporating and left me with a honey-colored oil. Not sure if there's any of the goodies in the oil, or how I would go about finding out.

Let it dry as much as possible and recrystallize in a small amount of anhydrous acetonitrile.

It's been drying all day and is starting to form crystals! Not nearly as much as I'd hoped, but still a substantial amount. I don't have acetonitrile. Am I right in thinking that I can recrystallize in IPA?

fractal

Subordinate Wasp

Posts: 110

Re: Short Question Thread 2.0

« Reply #358 on: April 11, 2013, 12:05:13 AM »

Yeah, there are a bunch of different solvents that will get the job done.